Method of setting wool textiles with ethanolamine



3,959,990 Patented Oct. 23, 1962 3,059,990 METHOD (OF SETTING WOOL TEXTILES WITH ETHANOLAMINE Nathan H. Koenig, El Cerrito, William L. Wasley, liberkeley, and Clay E. Pardo, in, Albany, Calif., assignors to the United States of America as represented by the Secretary of Agriculture N Drawing. Filed Nov. 3, 1959, Ser. No. 850,740 4 Claims. (Cl. 8-428) (Granted under Title 35, US. Code (1952), see. 266) A non-exclusive, irrevocable, royalty-free license in the invention herein described, throughout the world for all purposes of the United States Government, with the power to grant sublicenses for such purposes, is hereby granted to the Government of the United States of America.

This invention relates to and has as its primary ob ect the provision of novel methods for imparting to wool textiles durable creases, folds, pleats, or other structural arrangements as may be desired by the operator. Further objects and advantages of the invention will be evident from the following description wherein parts and percentages are by weight unless otherwise noted.

A simplified flow sheet illustrating the method follows:

Wool fabric I Apply solution containing about from 0.1 to by Weight of ethanolamine Arrange fabric in predetermined pattern, for example, pleats, creases or other desired fabric arrangement I Apply heat (about 85-15 0 C.) while fabric is constrained in predetermined pattern Product: Wool fabric provided with durable pleats, creases, or the like It is of course well known that garments of all types are provided with some sort of fabric arrangement, for example, pleats, creases, etc. Such deformations are conventionally produced by ironing the garment while constrained in the desired pattern. However, these arrangements are but temporary and when the garment is subjected to wear or is exposed to humid conditions the creases, pleats, etc., disappear leaving the garment in a shapeless condition. Materials such as starch are widely employed to obtain more durable creases. However, mpregnation of the textile with starch and similar materials has the drawback that the textile is rendered stiff and harsh so that it does not have the original characteristics of the untreated fabric.

The process of the invention affords many advantages not realized by prior techniques. Some of these advantages are explained below- In the first place, the fabric arrangements produced by application of the invention are durable, that is, they are essentially permanent in practical consideration. The treated textiles may be subjected to soaking in cold or even hot water without loss of the structure imparted thereto. Garments treated in accordance with the invention may be worn in the rain or subjected to other humid conditions without loss of pleats, creases, etc. The treated textiles may be subjected to dry cleaning or even mild washing in conventional aqueous soap or detergent formulations with little detriment to the creases, pleats, or other arrangements as may be present.

A most significant advantage of the process of the invention is that the durable arrangements are established Without impairing the desirable properties of the textile. That is to say, such properties as color, hand, elasticity, porosity, resiliency, strength, Wear-resistance, etc., are not harmed. For example, textiles treated in accordance with the invention exhibit essentially the same hand as the original fabric. This is in utter contrast to prior processes which depend for their eifectiveness on the application of shellac, gums, starches, resins, or other high-molecular weight coating materials. In those cases there is a substantial stifiening of the material so that the original hand of the fabric is impaired. The process of the invention does not involve constraining the shape of the textile fibers by any coating material but by a chemical rearrangement of the structure of the fibers into a new structural pattern.

The agent used in the process of the invention, ethanolamiue, is inexpensive, commercially-available, and nontoxic under the conditions of use. Particularly to be noted is the extraordinary effectiveness of ethanolamine in that it is operative in very low concentrations. This factor makes the process of the invention very economical.

Another advantage is that the textile arrangement is set merely by application of heat. No reducing agents, oxidizing agents, or neutnalizers are needed in the process of the invention. It is, of course, desirable to avoid the use of oxidizing and reducing agents since such compounds when applied to dyed wool often cause color changes and/ or bleeding of the dye. Also, by eliminating the need for any neutralizer, the process of the invention is simpler and more economical.

The process of the invention shrinkproofing treatments and in such cases of the effectiveness of the shrinkproofing is not impaired. Thus, for example, the setting process of the invention may be applied to textiles which are treated with polyepoxides and polyamides as disclosed by Pardo et aL, Amer. Dyestuff Reporter, May 19, 1958, pp. 333-338.

In applying the process of the invention, a solution of ethanolamine is distributed onto the textile, the textile is arranged in the desired pattern, and then while constraining it in such pattern heat is applied to set the arrangement.

The ethanolamine is applied to the textile in the form of a solution containing, by weight, about from 0.1 to 5%, preferably 0.25 to 2% of ethanolamine. By employing solutions containing not over about 5% of ethanolamine, the possibilities of degrading the wool or causing bleeding of dyes are minimized.

As the solvent for the ethanolamine solution, one may use water; a low molecular weight, oxygenated, volatile, organic solvent such as acetone, ethanol, or isopropyl alcohol; or a mixture of water and any of said organic solvents. Usually water alone is used as the solvent because of its eifectiveness and low cost. However, the use of volatile organic solvents with or without water may be preferred in instances when it is desirable to attain a more rapid drying of the textile after application of the ethanolamine solution.

The ethanolamine solution may be applied over the entire surface of the textile as by immersion, brushing, spraying, etc. Usually, however, it is preferred to apply the solution only to the area where the fibers are to be deformed. For example, in treating trousers in accordance with the invention, the solution is applied in a stripe or line along the length of the legs of the garment where the creases will be formed. It is obvious that by applying the solution only along the line where the textile is to be deformed, substantial economies are effected. Thus,

" in about 10 to 30 seconds.

not only is there a saving in the amount of ethanolamine required but there is also a saving of time and thermal energy during the heat setting step since only a limited area of the textile is treated.

The amount of ethanolamine solution applied to the textile is not critical. The solution exhibits a very potent effect in enabling the formation of durable textile arrangements and any amount thereof applied to the textile will result in an improvement over conventional creasing, pleating, or other type of fiber deformation produced by pressing with a hot iron or similar device. Also, there is no harm in using too much solution as any excess may be removed by wringing, water-washing, etc.

As stated above it is preferred to apply the ethanolamine solution along a line where the crease, pleat, or other configuration is to be formed. With such method of application, the amount of ethanolamine may be reckoned on the basis of volume per unit of linear distance. On this basis, then, it is preferred to deposit the solution in an amount to furnish at least 0.0005 ml. of ethanolamine per inch. More preferably to attain especially durable deformation the amount is at least 0.001 to 0.005 ml. of ethanolamine per inch. As noted above, no harm is done by using excessive amounts of ethanolamine solution. Ordinarily in practicing the invention, it is unnecessary to measure the amount of e-thanolamine solution to be applied-it is adequate to apply the solution in such amount as to moisten the fabric or at least the area where the crease, pleat, or other deformation is to be formed.

After applying the ethanolamine solution to the textile, the textile is arranged in the desired pattern. The arrangement may involve such manipulations as folding over sections of the textile, creasing, pleating, or shaping on suitable mandrels or dies. For example, in applying the process to garments, these articles are laid on a fiat surface with the desired areas folded over, creased, or otherwise arranged as conventional in preparing garments for pressing. Where more complex configurations are involved the textile may be compressed between dies having the desired shape. For example, ribbed effects may be obtained by constraining the fabric between dies having corrugated surfaces; pleated effects may be obtained by constraining the fabric between dies having mating V-shaped projections. Yarns may be crimped by compressing between corrugated surfaces. Further extensions of these principles will be obvious to those versed in the textile art.

-In any event, the textile while constrained in the arranged pattern is subjected to heat to set the textile fibers in the selected pattern. The heat treatment, or curing as it may be termed, is generally accomplished by contacting the textile with steam or with heated platens, rollers, dies, or the like. Also, the textile may be placed in an oven or subjected to radiation from infrared heaters or the like. For the establishment of pleats, creases and the like a conventional tailors steam press is quite satisfactory as the textile can be subjected to direct contact with steam while held in the selected pattern by the press pl atens. Generally, the heating, whether by steam or a hot roller, die, platen, etc., is at about 85 to 150 C. The time for cure is decreased with increasing temperature. Depending on the temperature the time for cure will be on the order of 5 seconds to 5 minutes. In any particular case, pilot trials may be conducted with different heating times and noting the durability of the arrangements in the treated textile by soaking it in water and observing its appearance. From such trials it is simple to determine the proper time of heating for the main batch of textile to be treated. Generally it is preferred to heat the ethanolamine-treated textile at a temperature of about from 140 to 145 C., in which case the deformation is set Also, heating by direct contact with steam is generally preferred as the penetration of the steam into the textile causes faster heating of the textile than is obtained with the case of hot platens, rollers, dies, or the like. Of course, a faster heating of the textile means that the time for setting is reduced.

The theory of the process is imperfectly understood. However, it is believed that during the heat treatment in the presence of ethanolamine, certain chemical bonds in the wool molecule are disrupted and then reformed into new patterns. By this molecular re-orientation the fibers are set in the position in which they are constained during the heat treating step.

A particular advantage in the use of ethanolamine for setting fabrics is that this compound is essentially nonvolatile. This means that solutions of the compound can be held for long periods of time without loss of the active component. Further, this non-volatile feature means that during the heating step, the ethanolamine remains in the area under treatment where it can effect the desired changes in fabric structure. Such action is a sharp contrast with the proposed use of such amines as trimethylamine, ethylene diamine, ethylamine, hydrazine, etc., for setting textiles. Such amines because of their volatility re vaporized during steaming so that they are dissipated from the field of treatment. In this connection it may also be noted that ethanolamine is less toxic than any of the volatile amines above nentioned and moreover because of its freedom from causing dermatitic reactions is commonly used in cosmetics, shampoos, etc. Ethanolamine is further characterized by having at most an armmoniacal odor in contrast to the repulsive, fishlike odors of the volatile amines. This factor is important in that the fabrics treated in accordance with the invention are free from the disagreeable odors associated with the volatile amines. Also, in contrast to known textile-setting agents, ethanolamine is free from the very objectionable odors encountered when the setting is performed with sulphur compounds such as thioglycollates, sulphites, and other agents producing hydrogen sulphide or sulfur dioxide.

It is to be emphasized that in the process of the invention no neutralizing agent is employed in connection with the ethanolamine solution. Thus this solution is employed at its autogenous pH which is generally about 11. The fact that no neutralizer is employed simplifies the process. Moreover, it would have been expected that ethanolamine in its unneutralized state would degrade wool especially when heated therewith. The fact that no degradation occurs is therefore a surprising aspect of the process of the invention.

The sequence of the operations of ([1) application of the ethanolamine solution and (b) mechanical arranging of the textile is not critical. Thus the textile may be treated with the solution, shaped to the desired pattern and heated while constrained in such pattern. On the other hand the textile may be shaped to the desired pattern, the solution applied, and the textile heated while constrained in such pattern. Moreover, although it is preferred to apply the solution to the textile prior to the heating step, this agent may be applied during the heating step. For example, the textile may be arranged into the desired pattern, then subjected to direct contact with a current of steam containing an entrained spray of ethanola-mine solution while the textile is constrained in the selected pattern.

Ordinarily the solution applied to the textile contains only solvent and ethanolamine. If desired a conventional wetting agent may be added to the solution to assist in penetrating and wetting the textile therewith. Suitable for this purpose are such agents as, for example: soaps, long-chain alkyl benzene sodium sulfonates, esters of sulfosuccinic acid, etc., typical examples being sodium oleate, sodium lauryl sulfate, sodium dodecane sulfonate, sodium alkyl (C -C benzene sulfonate, sodium dioctylsulfosuccinate, etc. Agents of the non-ionic type may be used, for example the reaction products of ethylene oxide with fatty acids, polyhydric alcohols, alkyl phenols and so forth. Typical of such agents are polyoxyethylene stearate, polyoxyethylene ethers of sorbitan monolaurate, isooctyl phenyl ether of polyethylene glycol, etc. Cationic agents may also be used as for example long-chain alkyl trimethyl ammonium chlorides, bromides, and methosulfates. Only a small concentration of wetting agent is needed, i.e., about 0.05 to 0.5% by weight of the solution.

The process of the invention may be applied to wool textiles in the form of threads, fibers, yarns, slivers, rovings, woven fabrics, knitted fabrics, felts, or garments made of woven or knitted fabrics. The wool textiles may be White or dyed goods and may be of all-wool composition or blends of wool with other textile fibers such as cotton, regenerated cellulose, viscose, animal hair, etc. Typical applications of the invention are: to provide garments with pleats, creases, or other arrangements customary in tailoring; to provide sheets of fabric with preformed pleats so that the product may be used for the fabrication of skirts, draperies, etc.; to produce crimp, twist, or other configuration in yarns, threads, and the like. Further applications of the invention will be obvious to those skilled in the art from the above illustrations.

The invention is further demonstrated by the following illustrative examples:

Example I A section of wool (tropical worsted, 4 oz./ sq. yd.) was cut into strips 50 cm. long and 4 cm. wide. Each strip was then folded in accordion fashion to provide seven pleats along the length of each strip.

Some of the folded strips were then treated with an aqueous solution containing 0.5% ethanolamine and 0.22% of a wetting agent (Triton X-l00, isooctyl phenyl ether of polyethylene glycol). In the treatment, this solution was applied with a brush along the line of each fold in an amount of about 0.3 ml. per inch. To provide controls, the remaining folded strips were not treated with the solution.

The treated and untreated strips, in the folded form, were placed in a tailors steam press. There they were pressed for 1 minute while subjected to direct contact with steam at about 140-l45 C. After steaming, the press platens were subjected to vacuum for 2 minutes to exhaust steam from the cloths.

To test the durability of the pleats, the following procedure was employed: After steam pressing each strip was suspended vertically by one end and the length of the strip (L) under its own weight then measured. The strips were then washed to ascertain the permanence of the pleats. The washing was done in a household agitatortype washer for 4 minutes at 38 C. in water containing 0.1% household detergent (Tide). After this washing the strips were air-dried while laid out on a flat surface. The strips were then suspended as before and their length (L) measured, The percentage permanence of the pleats is then obtained from the formula- The results obtained are tabulated below Percentage permanence= X 100 Permanence of Material: pleats, percent Treated with 0.5 ethanolamine 44 Control 17 Example 11 Samples of wool flannel (7 oz. per sq. yd.) were folded over and steam-pressed for about one-half minute. Each cloth was then treated with a solution containing a particular concentration of ethanolamine (as set forth below) and also between 0.01% and 0.05% of Triton Xl00. The ethanolamine solutions were applied along the creased portion of the cloths, applying about 0.1 ml. of solution per inch. The cloths were then pressed in a tailors steam press in which the steam supplied to the press was at -145 C. In each case, the cloths were pressed for periods varying from 5 seconds to 30 seconds while steam was flowing out of the press platens onto the cloths. The flow of steam was then cut off and suction applied to the platens to exhaust steam from the cloths. Suction was applied for 30 seconds.

The cloths were then removed from the press. It was observed that the creases were sharp. To test the durability of the creases, the cloths were washed as described in Example 1. After washing, the cloths were tumbledried for 20 minutes at about 65 C. in a household dryer. A control sample which was not treated with ethanolamine solution but which was steam pressed as were the other samples was also subjected to the washing tests.

After washing and drying, the cloths were examined to determined the character of the crease. The creases were rated on the following scales:

Excellent Good Fair Poor No crease The results are set forth below:

Concentration of Time of Run ethanolamine in steaming, Crease treating solution, seconds rating percent 15 Poor. 30 Excellent.

5 Poor. 15 Excellent. 30 Excellent.

5 Good. 30 Excellent. 30 Poor.

Example III In order to test the effect of the ethanolamine treatment on the tensile strength of the wool fabrics, the following experiments were carried out.

Samples treated as described in Example II were tested for breaking strength by the cut-strip method ASTM D39-49, measuring the force required to break the strip and noting whether the cloth tore at the crease or elsewhere.

The results are tabulated below:

Example IV As an additional test of the setting treatment, swatches of wool flannel were soaked over the entire: surface in ethanolamine solution and then pressed for 30 seconds with steam at 140-145 C. followed by 30 seconds under vacuum to exhaust the steam as described in Example II. The solubility of the treated strips as well as that of untreated control flannel were then determined as the percentage of material soluble in 0.1 N sodium hydroxide solution held at 65 C. for one hour. The following results were obtained.

Concentration of Alkali Run ethanolamine in solubility,

treating solution percent 11. 4 1.0 10. 9 None (controls). 10. 8, 11. 4

Example V A. A pair of brown wool trousers were rendered shrinkproof by the following treatment.

Polyepoxide A was a commercial product consisting essentially of diglycidyl ether of glycerol; polyepoxide B was a commercial product, essentially 2,2-bis(2,3-epoxypropoxyphenyl)propane; the polyamide was a commercial product being a condensation product of diethylene triamine and heat-dimerized unsaturated fat acid.

The emulsion was padded into the trousers with a wet pick-up of about 100%. The trousers were then cured in an oven at 125 C. for 30 minutes to cure the resin on the fibers.

B. A solution containing 1.5 ml. of ethanolamine and 98.5 ml. of distilled water was prepared. This solution was applied to the trousers, treated as described in part A, in the following manner. The solution was applied along the legs of the trousers following the line where the creases would customarily be formed. The solution was applied at a rate of about 0.1 ml. per inch. The trousers were then placed in a tailors steam press. There they were pressed for 30 seconds while subjected to direct contact with steam at about 140 C. After steaming, the press platens were subjected to vacuum for 30 seconds to exhaust the steam and dry the cloth.

The trousers so treated were worn for a total of 28 days over a period of two months during which time the creases retained their original sharpness and appearance. At the end of this period the trousers were washed in an automatic agitator-type home washer for 5 minutes at 38 C. in water containing 0.1% household detergent (Tide), rinsed, centrifuged and hung by the cuffs to air-dry. The creases following washing and drying were rated as excellent in appearance and sharpness. The dye on the trousers was not affected by the treatment. Measurements of the trousers after washing also indicated that the ethanolamine treatment did not harm the shrinkproofing effect of the polyepoxide-polyamide resin treatment.

Having thus described the invention, what is claimed is:

1. A method for imparting a stable set to wool textile material which comprises applying to a wool textile a solution of ethanolamine having a concentration about from 0.1 to 5% by weight, arranging the textile into a predetermined pattern, and while constraining it in such pattern subjecting it to heat to set it in the predetermined pattern.

2. A method of imparting a stable set to wool textile material which comprises applying a solution of ethanolamine having a concentration about from 0.1 to 5% by weight, to a selected area of a wool textile where the fibers are to be deformed, arranging the textile to deform said fibers according to a predetermined pattern, and while constraining the fibers in such pattern subjecting them to heat to set the fibers in the deformed position.

3. A method for imparting a stable set to wool fibers which comprises heating wool fibers in the presence of a solution of ethanolamine having a concentration about from 0.1 to 5% by weight while the wool fibers are constrained in a predetermined pattern.

4. A method for imparting a stable set to wool fibers which comprises applying steam to Wool fibers in the presence of a solution of ethanolamine having a concentration about from 0.1 to 5% by Weight while the wool fibers are constrained in a predetermined pattern.

References (Iited in the file of this patent UNITED STATES PATENTS 2,493,765 Le Compte Jan. 10, 1950 2,606,377 Edwards Aug. 12, 1952 2,955,958 Brown Oct. 11, 1960 FOREIGN PATENTS 540,086 Great Britain Oct. 6, 1941 775,486 Great Britain May 22, 1957 220,077 Australia Feb. 16, 1959 

1. A METHOD FOR IMPARTING A STABLE SET TO WOOL TEXTILE MATERIAL WHICH COMPRISES APPLYING TO A WOOL TEXTILE A SOLUTION OF ETHANOLAMINE HAVING A CONCENTRATION ABOUT FROM 0.1 TO 5% BY WEIGHT, ARRANGING THE TEXTILE INTO A PREDETERMINED PATTERN, AND WHILE CONSTRAINING IT IN SUCH PATTERN SUBJECTING IT TO HEAT TO SET IT IN THE PREDETERMINED PATTERN. 